四川盐边冷水箐岩体铂族元素的中子活化分析

四川盐边冷水箐岩体铂族元素的中子活化分析李晓林，汪云亮，肖庆帘（成都理工学院，成都６１００５９）关键词铂族元素，中子活化分析，镍锍试金为在川西地区寻找超大型硫化Ｃｕ－Ｎｉ－Ｐｔ矿床，需要对比剖析一些有关岩体。冷水箐岩体是研究对象之一。准确测定其铂族元...     

大洋多金属结核和深海沉积物标准物质中铂族元素的中子活化分析

采用镍锍试金预富集 中子活化分析方法,测定了大洋多金属结核标准物质ＧＳＰＮ ２、ＧＳＰＮ ３和深海沉积物标准物质ＧＳＭＳ ２、ＧＳＭＳ ３中的铂族元素;根据大洋样品成分特征,对常规的镍锍试金配方和熔炼条件作了改善;计算了活化分析中的铂族元素干扰核反应,校正了Ａｕ对Ｐｔ的二级干扰;选用羰基化镍粉配料,降低了铂族元素空白值。用国家一级标准物质ＧＢＷ０７１０２作了对照分析,结果与标准值相符。     

锍镍试金富集-等离子体质谱法测定煌斑岩中铂族元素

试金配料中适量加入铁粉,控制硫化铁在锍扣中的含量在20%~40%,获得的锍扣直接用水浸泡粉化后加盐酸分解,分解结束后趁热过滤,沉淀用1mL王水溶解,定容后上机测定,Cs作内标。改进后的方法空白水平进一步降低,检出限得到显著改善,分析流程简化。采用改进后的锍镍试金富集-等离子体质谱法测定了云南哀牢山金矿带煌斑岩和国家一级标准物质GBW 07288(GPt-1)、GBW 07290(GPt-3)中的铂族元素(PGEs)含量,方法检出限为0.001~0.01ng/g,精密度(RSD,n=5)为7.49%~16.6%。     

锍镍试金富集-电感耦合等离子体质谱法测定黑色页岩中的铂族元素

黑色页岩中碳、硫、镍等元素的含量很高,按照常规的锍镍试金熔剂配方不能形成较好的锍扣,影响铂族元素准确定值。本文通过调整试剂配方、优化操作流程等方式建立了黑色页岩中铂族元素的锍镍试金-电感耦合等离子体质谱(ICP-MS)测定方法。结果表明,加入适量硝酸钾可以将铂族元素回收率提高了大约10%。用盐酸溶解锍扣之后,溶液中仍然存在大量黑色沉淀,不易过滤和溶解,趁热在不断搅拌下加入2～3 mL三氯化铁溶液可以在很大程度上减少沉淀量,降低实验操作的难度和不确定性。方法检出限Ru为0.054 ng/g,Rh为0.040 ng/g,Pd为0.40 ng/g,Ir为0.032 ng/g,Pt为0.27 ng/g,Os为0.026 ng/g。精密度和准确度试验表明,该方法稳定可靠,可用于黑色页岩中铂族元素的准确测定。     

锍镍试金-电感耦合等离子体质谱法测定硫铁矿中铂族元素

锍镍试金常用于富集常规地质样品中的铂族元素(PGEs);而用于富集硫铁矿中的PGEs鲜有报道。硫铁矿中硫和铁的含量较高,采用常规的试金配方不能得到较好的锍扣,影响下一步样品的溶解和过滤。本文对锍镍试金-电感耦合等离子体质谱法测定硫铁矿中PGEs的流程进行改进。针对硫铁矿中硫和铁含量高的特点,在不减少称样量的情况下,调整常规锍镍试金中的试剂配方,获得了理想的锍扣和熔渣,使锍扣富集PGEs的能力达到最佳,且避免了由于反应时间过长而造成PGEs损失。同时利用硫化铁易剥落和粉化的特点,省去了锍扣的机械粉碎工序,简化了流程,避免了碎扣时的机械损失和样品间可能的交叉污染。结果表明,高含量的铁对PGEs的测定无显著影响。加标回收试验显示PGEs全流程回收率大于94%。按10 g取样量计算,方法检出限分别为Ru 0.018 ng/g,Rh 0.017ng/g,Pd 0.18 ng/g,Os 0.019 ng/g,Ir 0.013 ng/g,Pt 0.11 ng/g。实际样品分析和加标回收试验表明,改进后的锍镍试金-电感耦合等离子体质谱测定流程可以满足大多数硫铁矿中PGEs的测定要求。     

锍镍试金富集-等离子体质谱法测定西太平洋富钴结壳中的铂族元素

根据西太平洋麦哲伦海山富钴板状结壳样品的成分特征，对常规的锍镍试金配方作了改进；酌情减少捕集剂羰基镍的加入量，可显著降低铂族元素的空白值。富集后的样品，采用电感耦合等离子体质谱测定铂族元素（PGE）。其中，Ru、Rh、Pd、Ir和Pt用常规外标法测定，^175Lu作内标；Os用同位素稀释法测定。用国家一级标准物质GBW07290和GBW07291作监控分析质量的参考样，结果满足要求。     

微型核反应堆中子活化分析测定地质样品中铂族元素

采用镍铳试金预富集微型核反应堆中子活化分析测定地质样品中铂族元素，方法检出限低，ＲＳＤ〈１０％。     

锍试金富集贵金属元素：I.等离子体质谱法测定地质样品中痕量铂族元素

纯化了捕集剂，用锍试金结合Ｔｅ共沉淀富集，等离子体质谱法测定了地质样品中的铂族元素，全流程铂族元素回收率大于９４％，一次熔样可同时测定了６个铂族元素，按２０ｇ取样计算，方法检出限（ｎｇ／ｇ）分别为０．０２４，Ｒｕ，０．０１３，Ｒｈ，０．２０，Ｐｄ，０．０３３，Ｏｓ０．３９，Ｉｒ０．１２Ｐｔ；对标准ＧＰｔ－６平行测定５次，铂族元素相对标准偏差为１％（Ｏｓ）～８％（Ｐｔ）对不同类型标样进行测定，测得结     

地质样品中超痕量铂族元素的中子活化分析

文章概述了中子活化分析的基本原理和地质样品中超痕量铂族元素的中子活化分析方法。其中除介绍了样品的制备方法、照射和测量条件之外，还对地质样品中铂族元素放射化学分离方法进行了说细的讨论和评述。引用文献２４篇。     

锍镍试金-等离子体质谱法测定地球化学勘探样品中的铂族元素和金Ⅱ．分析流程空白的降低

对锍镍试金富集－等离子体质谱法测定贵金属流程中的试剂空白进行了检查，并对空白主要来源－捕集剂镍的各种纯化方法作了对比，提出了回收试金流程中溶扣后滤液中的镍循环使用。在有效降低空白的基础上，满足了化探样品所要求的0.0x ng/g级检出限，对超痕量贵金属标样分析结果与标准值符合。     

锍镍试金-等离子体质谱法测定地球化学勘探样品中的铂族元素和金Ⅰ．分析流程的简化

报道了一个改进的锍镍试金一等离子体质谱测定铂族元素和金的分析流程，用封闭溶解贵金属硫化物滤渣与同位素稀释法测锇相结合，解决了包括锇在内的全部铂族元素和金的测定，避免了锇的蒸馏分离和（或）单独测定，简化了分析流程，以适应大批量化探样品的要求，用所拟方法分析了标准物质中铂族元素和金，其结果与参考值相符。     

Platinum-Group Elements and Gold Determination in NiS Fire Assay Buttons by UV Laser Ablation ICP-MS

The direct analysis of nickel sulfide fire assay buttons by UV laser ablation ICP-MS was used to determine the platinum-group elements and gold in the following reference materials: UMT-1, WPR-1, WMG-1, GPt-4, GPt-6 and CHR-Bkg. The instrument was calibrated with buttons prepared using quartz doped with the appropriate standard solutions. Analytical precision (RSD) was generally better than 10%, although occasional higher RSDs may infer local heterogeneities within nickel sulfide buttons. Good or excellent agreement was observed between analysed and reference material values except Rh in UMT-1 and WMG-1, which suffered an interference from copper. Detection limits calculated as 10 s quantitation limits were Au (1.7 ng g⁻¹), Pd (3.3 ng g⁻¹), Pt (8.3 ng g⁻¹), Os (1.3 ng g⁻¹), Rh (1 ng g⁻¹), Ru (5 ng g⁻¹) and Ir (0.7 ng g⁻¹).     

Comparison of Recoveries by Lead Fire Assay and Nickel Sulfide Fire Assay in the Determination of Gold/ Platinum/ Palladium and Rhenium in Sulfide Ore Samples

We compared the recovery of gold, palladium and platinum by two fire assaying procedures, using nickel sulfide and lead as collectors. The presence of appreciable amounts of sulfide minerals in the sample caused interferences in both procedures. An in-house reference sample, a reference sample of high-grade sulfide ore and samples of high sulfide content from the Recsk porphyry copper ore in Hungary were analysed by both methods. The elements were determined by inductively coupled plasma-atomic emission (ICP-AES) and/or inductively coupled plasma-mass spectrometry (ICP-MS). It was found that for the sulfide ore samples, the recoveries of Au and Pd are sometimes lower by nickel sulfide fire assay than by lead fire assay. Recovery of Re by nickel sulfide fire assay was found to be low: the average recovery of five repeated analyses of the reference sample NIST SRM 330 was 9% with a relative standard deviation of 48%. Increasing the amount of S in the fusion flux gave better recovery.     

Determination of the Platinum-Group Elements and Gold in Twenty Rock Reference Materials by Inductively Coupled Plasma-Mass Spectrometry (ICP-MS) after Pre-Concentration by Nickel Sulfide Fire Assay

The platinum-group elements (PGE) and gold have been determined in twenty international rock reference materials by inductively coupled plasma-mass spectrometry (ICP-MS) after pre-concentration by a nickel sulfide fire assay. It was possible to achieve determination limits for a 50 g sample that ranged from 1 pg g^-1 (Rh) to 23 pg g^-1 (Au). Compared to published certified and recommended values for rock reference materials, the trueness of the method was found to be good. However, in some cases we observed large deviations for all elements in the sub 10 ng g^-1 range within individual reference sample splits. Our results show that the PGE and Au are inhomogeneously distributed in the reference materials analysed here, where they are present in low concentrations, using 50 g test portions.     

中子活化法测定铝材料中杂质元素

测定了用作反应堆的铝材料中Ｆｅ,Ｃｕ,Ｚｎ,Ｌａ,Ｓｍ,Ｍｏ,Ｈｆ等２３种杂质元素含量。对于Ｔｉ和Ｎｉ采用超热中子活化法,其它元素采用热中子活化法。实验测得了裂变系数,用于扣除Ｕ对Ｃｅ,Ｎｄ,Ｚｒ,Ｌａ,Ｓｍ等元素的干扰,计算了铝材中各杂质元素的探测极限,该方法精密度,对几个标准参考物质的分析结果与推荐值相符。